CS248480B1 - A method for continuously conducting a reaction of ammonium nitrate ammonium nitrate and / or urea with sulfuric acid and / or phosphoric acid and an apparatus for carrying out this process - Google Patents

Abstract

The solution relates to a method and a device for continuously conducting the reaction of ammonium nitrate and/or urea ammoniates with sulfuric and/or phosphoric acid, which is useful primarily in connection with the production of granular compound fertilizers. The reaction between the ammonia contained in the ammonia and sulfuric and/or phosphoric acid occurs as a result of the contact of the ammonia and the acid in front of the reaction mixture layer. Intensive mixing of the reaction mixture and continuous removal from the reaction environment is achieved primarily by the formation of a vapor-gas mixture, which under the reaction conditions constitutes at least 70 volume percent of the reaction mixture. The contact of the reacting components preferably occurs below the reaction mixture layer. Water is preferably added to the reaction mixture. The device for the continuous reaction of ammonium nitrate and/or urea with sulfuric and/or phosphoric acid consists of a vertically situated reactor body, which is connected by a horizontal part to a distributor of the reaction mixture. The water supply of ammonia and sulfuric and/or phosphoric acid flows into the lower part of the vertically situated reactor body. The water supply also flows into the reactor, if applicable.

Description

248480

The present invention relates to a process for continuously reacting ammonia, ammonium nitrate and / or urea with sulfuric acid and / or phosphoric acid, useful in particular for the production of granular multi-component fertilizers and apparatus for carrying out this process.

Solubility of some inorganic salts, especially nitrates and some of the anorganic compounds (urea, thiourea)

Sol - a type of nitrate - in NH4NO3

Ca (NO3) 2

NaNChKNO3 vine and the like in a concentrated liquid ammonia is comparable and sometimes higher than in water. KLEVKE, V. A. - LE-VIN, I. A. - PETRJAEVA, D. A. - TOŠCEV, A. F .: "Jews abotnyje udobrenia", Moscow, Izd. Chimija 1973 gives the following values for some nitrates in water and in liquid (100% ammonia at 25 ° C):

Solubility (g / 100g) in water in liquid. (100% NH 3 NH 3 3 587803.5 986.7 103.4 2 0901 380927382.5 For example, BERGMAN, AG - MOROZ, KK was investigated by studying the liquids obtained by reacting anhydrous, ammonia gas with solid ammonium nitrate. 1967, pp. 551-555. These authors suggest that two crystalline compounds, NH1NO3.2NH5 and NH4NO3, NH3, can be expected to be present in the NH4NO3-NH3 system at a temperature range of -15 to +25 [deg.] C. the detailed results of the study of phase equilibria in the NH3-COfNH2Ja-NH4NO3 system.

Due to the relatively high content of nitrogen in the solutions of said compounds in concentrated ammonia, in the so-called ammonia, these are used as pressure nitrogenous fertilizers for direct application and serve as a source of nitrogen in the production of liquid non-pressurized and in particular some types of multi-component fertilizer granules. The use of ammoniacs is widespread in the main in connection with the production of granular fertilizers coated with so-called integrated technologies which allow the production of high-concentration granular fertilizers (GVH).

Rationally combining chemical and mechanical technology in one process allows for the production of excellent GVH types, which typically exceed agrochemical and physico-mechanical properties by the level of GVH prepared by the decomposition of phosphate by nitric acid, or by combining it with other mineral acids.

Good results in the production of GVH by integrated technologies are achieved by the THÚ-RING process, which uses ammonium nitrate ammonium nitrate as a source of nitrogen, containing 55 to 63 + 1.5 wt. 20 to 26 + 1.2 wt. % NH3 and 17 to 19 + 2.7 wt. % of water, so that the total nitrogen content of the feedstock process usually corresponds to 38.5 to 40.6+ 1 wt. % N. V is of interest in the bonding of the free ammonia contained in the ammonia, and it is also necessary to incorporate some of the mineral acids, usually sulfuric acid, phosphoric acid or mixed acids, into the production process of GVH. Addressing the ammonia and acid feeds into the GVH production process in the integrated technology of the type mentioned has a profound effect on the agronomic value of the product (in particular the phosphorous efficiency), safety and operational reliability of the technology; compliance with the ammonium acetate consumption standard; nitrogen, chlorine and fluorine emissions; physical-mechanical properties of the granulate and the like. The source of the overwhelming majority of the aforementioned difficulties is the thermal decomposition of ammonium nitrate contained in the ammonia, to which the liberated neutralizing heat can be released. The thermal decomposition of NH 4 NO 3 depends on the temperature, its physical state, the presence of oxidizing and catalytically admixing impurities and the like. The literature suggests that above 150 ° C, an endothermic decomposition of NH 3 NO 3 and NH 3 can be observed:

NH 4 NO 3 - NH 3 + HNO 3 AH ° 2i 31 = 9 967 I

With careful heating above 185 ° C, decomposition of NH4NO3 occurs according to the equation:

NH 4 NO 3 -> 2 H 2 O + N 2 O AH ° 29i = - 2 107 J

Above 235 ° C, decomposition of NH 4 NO 3 takes place already autocatalytically and can lead to explosion. Rapid heating to 400-500 ° C causes explosive decomposition according to reaction: NH4NO3 - Nz + V2 02 4- 2 H20

AH ° 201 = - 6,800 J

The explosivity of NH4NO3 is greatly enhanced by the presence of inorganic substances, easily O-oxides and metals in the powdered form (Cu and Znj act most dangerously. Explosive thermal decomposition causes its cause that decomposition products do not act catalytically. They mainly produce nitrogen oxides and partly water vapor. Partial decomposition of KCl to hydrogen chloride can occur as a result of contacting the feed of strong mineral acid [HsSO4] with potassium chloride, usually used as a source of potassium. In the presence of substances that remove water (eg concentrated H2SO4), nitrogen oxides (mainly N2O: l) can react with chlorine by the nitrosyl chloride chloride - NOCI, which is marked by the eudothermic compound:

N 2 O 3 + 2 HCl -> 2 NOCl + H 2 O

By reacting nitrogen dioxide with sulfuric acid, it can also ignite in the system of interest by the equation:

N, O i 4- 2 H 3 SO 4 - 2 (NO) (HSO 1 + H 2 O hydrogen nitrosyl bisulfate, which is commonly referred to as nitrosylsulfuric acid in the presence of some gaseous fluorine compounds that can be formed by decomposition in the system under study) of the phosphorus raw materials used, I can carry out reactions of the type: 2 N 2 O 5 + S 1 F 4 -4 2 HF 2 HNO 3 + + (NO 2) 2 (SiFe), the product of which can be nitrites (nitrile fluorosilicate).

The imperfect distribution of the ammonia in the granulation mixture may also result in the subsequent flocculation of the phosphoric raw material used (calcium and / or ammonium phosphates), resulting in significant reductions in the agronomic value of the phosphorus fertilizer. In order to solve the above problems, by the manufacturers of GVH, integrated technologies will be able to optimize mainly the method of supplying ammonia and the mineral acid used. In summary, the following systems have been used to address this problem in practice, or the following systems have been verified at least under operating conditions: - solution of ammonia supply and acid-vapor pairs of flexible feeds to granulated granulation; - batch or continuously guided reaction of the ammonia with the used mineral acid in a stirred neutral reactor of the boiler-type extra-granulation process; The use of continuously operating pre-neutralizing flow reactors, which are incorporated in the granulating drum, or located in its close proximity and in the interior thereof.

The first two of these systems are characterized by a number of shortcomings, including the following: - low degree of operational certainty; - low energy efficiency :; - high maintenance requirements for technological equipment; - problematic adherence to the required ratio between the ammonium acetate and the mineral acid (mainly in the case of solutions to the distribution of multiple flexible feed systems); - low level of occupational safety with regard to the possibility of self-igniting explosive or toxic substances; - the content of separately monitored gaseous ex-halates in the off-gas from the granulator; - Phosphorus retrogradation; - uneven composition of the produced granulate and some others.

The most significant disadvantages of the existing methods of incorporating liquid amino acids and mineral acids into the granulating mass include the undesirable side reactions between the individual components occurring in the granulation process, which are the source of respiratory and pathologically active exhalations, high corrosive compounds, and can also cause spontaneous burn up to sudden exfusion. The purpose of the pre-neutralization of the ammonia with the respective mineral acid (usually H2SO4, H3PO4, respectively their granules) is to prevent the over-acidification of the granulation mass, thereby virtually eliminating the possibility of these undesired side reactions. The pre-neutralizer must be designed to provide perfect contact of the reagents and to suppress the decomposition in the ammonium nitrate of the ammonium nitrate contained in the NH4NO3 by the mineral acid used.

Up to now, in the operating conditions of continuous-flow continuous reactors for ammonium nitrate neutralization and / or urea mineralization, even though they have progressed in solving the discussed problem, they have a number of drawbacks. in the production of GVH, it did not solve all the problems of the monitored area at the required level. In the past, pre-neutralized reactors, at least (brief) two, which have already been tested under the operating conditions of GVH manufacturing practice, can be cited here. The basis of the function of the first was

? 4 8 4 8 To mogenize the reactants (ammonium nitrate ammonium nitrate and sulfuric acid) after spraying them onto a stable Teflo-New cone.

A second type of pre-neutralizer being tested used to mix the ammonia with the acid-free gravitational flow of reactive components along alternately placed baffles built inside the vertically situated reactor body. From an orientation experiment, using a full-frame model apparatus (see example), said method of continuously reacting ammonium nitrate ammonium nitrate with sulfuric acid does not create the prerequisites for the efficacy of the reactants and creates favorable conditions for the formation of self-igniting more reactive products.

The above problems are solved by a process for continuously conducting the reaction of ammonium nitrate ammonium and / or urea with phosphorous and / or phosphoric acid, which can be used in particular for the production of granulated multi-component fertilizers, consisting in the reaction between ammonia contained in ammonia and acid sulfur and / or phosphorous, as a result of the contact of the ammonia and the acid with the pre-layer of the reaction mixture, intensive mixing of the reaction mixture and continuous discharge from the reaction medium is mainly achieved by the formation of a vapor-gas mixture which, under the reaction conditions, constitutes at least 70% by volume of the reaction mixture wherein the heterogeneous reaction mixture formed by the reaction yields from the reaction medium a linear velocity of 3 to 125 m.s. -1. Furthermore, it has been found that the particular advantageous contacting of the reactants - ammonium acetate and one or both acids - occurs under the reaction mixture layer. In order to adjust the optimum temperature ratios for neutralization, flow velocity and thus the mixing efficiency of the reaction mixture, as well as to provide a highly efficient dispersion of the absorbent with the plant nutrient content in the granulation mass, it has proven to be advantageous to add to the reaction mixture. the mixture of water in the liquid and / or vapor phase, or added to the reaction mixture an aqueous solution and / or aqueous suspensions of nitrogen and / or potassium containing. This water, steam or water-containing component can be introduced into the reaction medium separately or together with one of the reactants.

A device for continuously conducting the reaction of ammonium nitrate and / or urea nitrate with sulfuric acid and / or phosphoric acid according to the invention, particularly in connection with the production of granular multi-component fertilizers (FIG. 1), consisting of a sulfuric acid feed 1 and ammonium phosphate and / or ammonium nitrate ammonium nitrate and / or urea feed 2, which extend into the lower portion of the reactor 3, vertically situated, the horizontal connecting portion 4 connected to the reaction mixture distributor 5, wherein In addition, a water inlet 6 or a vapor or aqueous solution and / or a suspension of nitrogen and / or phosphorous inorganic salts and / or potassium may be added to the reactor.

In continuously conducting the reaction of ammonium nitrate and / or urea with sulfuric acid and / or phosphoric acid and using the apparatus according to the invention, the feed 1 leading into the vertically situated reactor body 3 in its lower end is carried out. the sulfuric acid and / or phosphoric acid is metered in and the second feed 2, which also enters the vertically aligned portion of the reactor body 3, is charged with ammonium nitrate ammonium and / or urea. The contact of the reacted reactants causes a rapid neutralization reaction associated with the release of the reaction heat and thus the formation of water vapor. The formation and gradual overheating of the water vapor causes the reaction mixture to significantly increase its volume resulting in a highly turbulent mixing the reaction mixture and also discharging it from the vertically settled so-called mixing portion 3 of the reactor to the coupling portion 4 of the reactor to its end portion formed by the vapor-liquid distributor 5. The manifold 5 may have a variety of shapes and may open the granulation mass, into the solid component feed and / or into the recycle port, or above the granular surface. Particularly advantageous has been its placement in the granulation mass of the granular material produced in the pelletized granulate. When placing the outlet 5 into the granulation mass (at a depth of 50 to 300 mm), it is advantageous to have a stretched shape (e.g., oval, irregular rectangle, ellipse, etc.) over at least that portion of the distributor 5 which is immersed in the granulation mass. in the direction of rotation of the granulator, or if a portion of the submerged granulated mass is provided with a knife. If the outlet of the vapor-liquid reaction mixture is discharged into the space-solid granulating mass, it is desirable to shape the dispenser 5 and position it so that the longer of its cross-sectional axis is located in the direction of the granulating drum axis or in the direction of the granulation mass flow. . In such a case, it is usually sufficient if the divider 5 is designed as an extension of the horizontal connecting portion 4, which is terminated by a long slit forming its own divider 5, wherein the slot is situated in the direction of the axis of the granulating drum and ensures a fine dispersion of the vapor-liquid the reaction mixture over the surface of the granulating mass.

It is also advantageous if a water and / or steam inlet and / or steam and / or steam are discharged into the upper part of the vertical mixer 3 and / or in one of the connecting horizontal parts 4 and / or 4 8 4 9 9 10 in the reaction mixture. or a device comprising components containing nitrogen and / or phosphorus and / or potassium.

By the addition of a suitable amount of water and / or water vapor and / or an addition of a liquid component containing nitrogen and / or phosphorus and / or potassium (e.g., an absorbent solution or a suspension of the final process wash), the following can be achieved: The desired reduction in the temperature of the reaction mixture and thus a significant inhibition of the undesired side reactions! type:

t> 150 ° C NH 1 NO 3 -------- NH 5 j-HNO 3

ΛΙΓ 1 = + 9 967 J

t> 185 ° C

NH 4 NO 5 -------- N 2 O + 2H 2 O

Ϊ́ ° 29ΐ = —2,107 J

t> 218 ° C (----- NH4HSO1 + NHs - Improvement of conditions for binding of free ammonia to the granulation mass and formation of favorable conditions for the expansion of the vapor-liquid reaction mixture above the granulation layer; continually removing eventually formed solids of the solidified liquid-melt phase of the reaction mixture from the internal walls of the reactor and the orifice of the manifold, as well as some other beneficial effects on the course of the technological process. EXAMPLES 1 - 7 In order to study the basic conditions of the reaction of ammonium nitrate ammonium nitrate with sulfuric acid, as well as the knowledge of the essential technological properties of the resulting liquid phase reaction, the first phase seam is made by a series of laboratory The batches of ammonium nitrate ammonium acetate containing 25.88 wt. % free NH 3 55.34 wt. % NH 1 NO 3 40.71 wt. % total nitrogen (as N)

The sulfuric acid used contained 92 wt. % MH-H2SO4.

The laboratory apparatus consisted of a six-neck thermos flask of about 1 dm 3, a doctor through the holes in the cork stopper of the two glass-dispenser glass dispensers, a glass double-wing stirrer and a thermometer.

During the experiments, the bound amounts of the two mixed components were approximately simultaneously and simultaneously released at the same time, by opening the glass coils, with efficient mixing into the thermos while aiming to determine the maximum reaction temperature reached mixture.

The first 4 of these bleach experiments were conducted so that the amount of blended components (ammonia and H2SO4) used approximated neutralization of free ammonia in the senses: NH3 + H2SO4 -> NH4HSO4

During further experiments, the dosing of the reactants was adjusted so that the free ammonia in ammonia was neutralized to the second stage of the dosed amount of H 2 SO 4.

An overview of the basic results achieved during laboratory experiments of this serum is contained in Table 1.

Although small-scale indicative indicative characteristics and their results are likely to be obstructed by the experimental error caused by the uncontrollable leakage of a portion of free ammonia from the ammonia used, their results have contributed to the effective avoidance of the next quarter of operational technology research in the subject matter. . and a 'ta c

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In order to illustrate some of the advantages of the present invention, we present, in this example, the results of a continuous run of a nitric ammonium ammonium ammonia neutralization feed containing 26 + 1.2 wt. % free NH 3, 55 + 1.5 wt. % NH 4 NO 3 and 19 + 2.7 wt. % water by sulfuric acid containing 92 wt. % MH-H2SO4 in the top-flow reactant flow-through column.

The apparatus used consisted of two reservoirs (ammonia and sulfuric acid) placed on the scales, from a piston-dispensing pump and Bran-Lubbe with a porous cellular dosing head, used for the dosing of H2SO4, from the peristaltic-hose dosing pump and Ba-chofen used for dosing. from a vertically located glass column with a total height of 1,250 mm and a 50 mm filling filled with a nonorganized ceramic filling (Raschig rings d = 10 mm) and a steel barrel of volume 200 dm 1 2 3 into which the bottom end glazed filler The column provided with the withdrawal of the gaseous reaction products by means of a fan through a water-scrubbed absorption column. The column of the lower third layer of the filler and thus the reaction mixture was placed in the steel barrel forming the collection product of the reaction. mercury thermometers (0-250 ° C).

On average, 667.7 g of NH 4 NO 3 tartrate are already dispensed into the apparatus of the above type with separate feeds extending above the filler layer and 500 g tq of H 2 SO 4 containing 92 wt. % MH-H2SO4.

Practically instantaneous upon reaching the contact reactants on the filler layer and at the top of the filler and in the free space above the filler, a continuous flame of orange-brown fabric appeared, which had an upper-violet border in the upper. The flame associated with the formation of the pyrophoric decomposition products of the study reaction did not disappear throughout the duration of the experiment (about 40 min), and its size and intensity were directly related to the change in dosage of the amount of ammonium niobate.

The lower reaction temperature of the reaction mixture varied from 190 to 220 ° C, depending on the variations in the dosage of ammonia, with a temperature of up to 220-230 ° C being measured on the second thermometer (before the reaction mixture went into steel).

It has been observed that during the experiment the reaction mixture - a strongly foamed melt - gradually increased its viscosity and loose flow capability. Likewise, the vapor-gas mixtures of the flocculent white (water vapor) are increasingly staining yellow-brown from the gaseous decomposition products. After completion of the ammonia and acid dosing, two samples of the solidified molten reaction mixture were removed from the tubular section after the filler, in which the content of the determined components was determined by analysis:

Determined component Sample number: 1 2

Total nitrogen (wt% N i 24.70 24.56 Ammoniacal nitrogen (wt% N i 19.18 18.98

The total sulfur (wt% S) of 15.70 15.80 from the pipeline route used to aspirate the vapor-phase portion of the reaction mixture from the reaction mixture collection reservoir was insulated with brown-red powder condensate in which sample (no. 3) the content of the components analyzed has been determined: - total nitrogen content:

27.99 wt. % N - Ammoniacal nitrogen content:

14.38 wt. % N - total sulfur content:

0.51 wt. % S - total iron content: 5.44 wt. % Fe.

The acidity of the individual samples, expressed as pH of 1% solutions in the distilled water (pH0.6), was:

Sample No. pH 1 3.0 2 2.7 3 6.6 Examples 9 and 10

The process of continuously conducting ammonium nitrate neutralization with an acid-acceptor according to the invention has been verified for a long time on a model quarter operating apparatus, the critical parts of which were constructed from a standard 25 mm technical glass. The apparatus consisted of a glass spacer - the "T" fittings, to which the supply of reactive components - ammonia (s) were solved by means of stainless steel tubes (ČSN 17 246; d = 12X1 mm), sealed with rubber stoppers. sulfuric acid (bottom neck so that the mouth of the metal tube reached about 50 mm above the ammonia orifice). The specified T-piece was fitted with a vertically positioned glass tube (Ms 25 mm; 1 = 300 mm) terminated at the top of the "T" -shaped tube, which was used to install the thermometer into the vertical, by means of a rubber seal and standardized screw coupling. and a glass 248480 1314 tube (Ms 25 mm; 1 - 1000 mm) extending on the opposite side of the normalized bead to the metal collecting container of the reaction product. The dosing of ammonia and acid, such as removal of the vapor-gas mixture from the product reservoir, was solved by analogy with the procedure described in Example 8. The specification of the raw materials used, as described in the previous example. The weight ratio of the ammonium amide (ADA) and sulfuric acid dosed was prescribed equally for both experiments and should be equal; tq ADA / tq H 2 SO 4 = 1.335; wherein the actual dosage amounts of the reactants during both experiments are equal to:

Experiment No. Dose Quantity (kg tq. H_1) ADA H2SO4 9 41.2 32.2 10 98.0 69.6

During the two quarters of the experiments, no phenomena were observed that would indicate a significant thermal decomposition of the ammonium niobate. The temperature of the reaction mixture as measured by the vertical-mixing step was, in the case of experiment No. 9, 172-174 ° C and the temperature of the reaction mixture varied between 165-172 ° C during experiment no.10.

Under the indicated reaction conditions, it can be assumed that the weight ratio of the liquid-melt phase to the vapor-gas mixture in the reaction product was close to 85/15 = 5.7; wherein the volume of the resulting gas-vapor mixture in the case of Test No. 9 is about 6.5 dm 3. s-1, and for the # 10 condition, it can be concluded that its value was close to 14.8 dm 3. s_1.

It can also be further assumed that the volume of the liquid-melt phase from the total volume of the reaction mixture in part No. 9 was about 0.15% by volume and in the experiment. 10 even only about 0.06 vol%. With the type of glass tube part used (Ms 25 mm; P = 490.6 mm 2), it can be assumed that the average mass linear velocity of the reaction mixture in the apparatus used was approximately equal to 13.2 m. 30.1 m. s-1 (during run # 10).

Due to the high mass linear flow rate of the reaction mixture, the high-turbulence mixing of the reaction mixture over the sulfuric acid orifice (Fig. 2) and the high degree of liquid phase dispersion in the vapor-gas phase were highly efficient. reaction mixture of its outlet from the tubular portion of the apparatus.

During the two quarters of the experimental attempts to exit the reaction mixture from the tubular apparatus to the collecting tank, a number of melt samples are taken whose moderate chemical composition is as follows:

Determined Component Melt from Experiment No. 10 10 Total Nitrogen Content (wt% N) 23.34 24.78 Ammoniacal Nitrogen Content (wt% N) 17.66 18.66 Total Sulfur Content (wt% S) 16.48 15.46

The aqueous extract of the sampled samples melted the acidic reaction - pH of 1% of the melt in distilled water (pH 0 6.05) bolopre of the sample from Experiment 9 equal to 2.1, and the number 10 was averaged pH2.4.

Claims (4)

13 16 243430 OBJECT A process for continuously conducting ammonium nitrate and / or urea nitrate reaction with sulfuric acid and / or phosphoric acid for the production of multi-component fertilizer granules, characterized in that the reaction between ammonia contained in ammonium nitrate and sulfuric acid and / or phosphorus The reaction mixture is effected by contacting the ammonium acetate and the acid in the presence of water in front of the reaction mixture layer, the reaction mixture being vigorously stirred and yielding from the reaction medium a linear velocity of 3 to 125 m. with a vapor-gas mixture formed by the reaction and vapor-gaseous, under reaction conditions, a minimum of 70% by volume of the heterogeneous reaction mixture will be formed. 2. A process according to claim 1, wherein the reactants are contacted under the reaction mixture layer. VYNALEZU 3. Process according to claim 1, characterized in that a liquid and / or vapor phase or aqueous solution and / or an aqueous suspension of nitrogen-containing inorganic salts and / or phosphorus and / or potassium is added to the reaction mixture. , which is introduced separately into the reaction medium, or together with one of the reactants. 4. Apparatus according to any one of claims 1 to 3, characterized in that the sulfuric and / or phosphoric acid feed (1) and the inlet (2J ammonium nitrate ammonium and / or urea to the lower part of the vertically situated one). a reactor (3) which is connected by a horizontal portion (4) to the reaction mixture distributor (5), whereby a feed (6j of water and / or aqueous vapor or an aqueous solution and / or or a suspension of inorganic salts containing duo and / or phosphorus and / or potassium 1 sheet of drawings